Micellar electrokinetic capillary chromatography for the determination of Viagra and its metabolite (UK-103,320) in human serum
Micellar electrokinetic capillary chromatography (MEKC) was investigated for the determination of Viagra (sildenafil citrate, SC) and its metabolite (UK‐103,320) in human serum in a concentration range of clinical interest. For MEKC, human serum samples spiked with SC and UK were obtained directly a...
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| Veröffentlicht in: | Electrophoresis 2001-06, Vol.22 (10), p.2004-2009 |
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| creator | Nevado, Juan J. Berzas Flores, Juana Rodríguez Peñalvo, Gregorio Castañeda Fariñas, Nuria Rodríguez |
| description | Micellar electrokinetic capillary chromatography (MEKC) was investigated for the determination of Viagra (sildenafil citrate, SC) and its metabolite (UK‐103,320) in human serum in a concentration range of clinical interest. For MEKC, human serum samples spiked with SC and UK were obtained directly after elution with methanol from a tC18 cartridge. The extract was evaporated and regenerated in a solution 1 mM of phosphate buffer (pH 12.3) which contained a methanol percentage of 20% that was analyzed using phosphate buffer (pH 12.3, 10 mM) containing 30 mM sodium dodecyl sulfate (SDS) as separation electrolyte and a fused‐silica capillary. This method gave satisfactory interday precision with respect to migration times relative standard deviation (RSD |
| doi_str_mv | 10.1002/1522-2683(200106)22:10<2004::AID-ELPS2004>3.0.CO;2-W |
| format | Article |
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Berzas ; Flores, Juana Rodríguez ; Peñalvo, Gregorio Castañeda ; Fariñas, Nuria Rodríguez</creator><creatorcontrib>Nevado, Juan J. Berzas ; Flores, Juana Rodríguez ; Peñalvo, Gregorio Castañeda ; Fariñas, Nuria Rodríguez</creatorcontrib><description>Micellar electrokinetic capillary chromatography (MEKC) was investigated for the determination of Viagra (sildenafil citrate, SC) and its metabolite (UK‐103,320) in human serum in a concentration range of clinical interest. For MEKC, human serum samples spiked with SC and UK were obtained directly after elution with methanol from a tC18 cartridge. The extract was evaporated and regenerated in a solution 1 mM of phosphate buffer (pH 12.3) which contained a methanol percentage of 20% that was analyzed using phosphate buffer (pH 12.3, 10 mM) containing 30 mM sodium dodecyl sulfate (SDS) as separation electrolyte and a fused‐silica capillary. This method gave satisfactory interday precision with respect to migration times relative standard deviation (RSD < 1%) and linear responses for the concentration ranges investigated (0.50–3.50 mg L–1 for the compound SC and 0.90–4.60 mg L–1 for UK). An intraday RSD (n = 5 graphs) between the slopes of the calibration graphs was acceptable (6.40%) for SC and (3.37%) for UK. A satisfactory interday precision between slopes was also obtained (RSD 4.10% for SC and a RSD 2.72% for UK) which demonstrated the ruggedness of this method. Detection limits (S/N = 3) were about 200 ng/mL for both compounds in human serum. MEKC was shown as a good method with regards to simplicity, precision and sensitivity.</description><identifier>ISSN: 0173-0835</identifier><identifier>EISSN: 1522-2683</identifier><identifier>DOI: 10.1002/1522-2683(200106)22:10<2004::AID-ELPS2004>3.0.CO;2-W</identifier><identifier>PMID: 11465499</identifier><language>eng</language><publisher>Hoboken: Wiley Subscription Services, Inc., A Wiley Company</publisher><subject>Electrophoresis, Capillary - methods ; Electrophoresis, Capillary - statistics & numerical data ; Human serum ; Humans ; Male ; Micellar electrokinetic capillary chromatography ; Micelles ; Osmolar Concentration ; Phosphodiesterase Inhibitors - blood ; Phosphodiesterase Inhibitors - metabolism ; Piperazines - blood ; Piperazines - metabolism ; Purines ; Pyrimidinones - blood ; Pyrimidinones - metabolism ; Sildenafil Citrate ; Sildenafil citrate (Viagra) ; Sildenafil metabolite (UK-103 ; Sildenafil metabolite (UK‐103,320) ; Sodium Dodecyl Sulfate ; Sulfones ; Temperature</subject><ispartof>Electrophoresis, 2001-06, Vol.22 (10), p.2004-2009</ispartof><rights>Copyright © 2001 WILEY‐VCH Verlag GmbH, Weinheim, Fed. 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Berzas</creatorcontrib><creatorcontrib>Flores, Juana Rodríguez</creatorcontrib><creatorcontrib>Peñalvo, Gregorio Castañeda</creatorcontrib><creatorcontrib>Fariñas, Nuria Rodríguez</creatorcontrib><title>Micellar electrokinetic capillary chromatography for the determination of Viagra and its metabolite (UK-103,320) in human serum</title><title>Electrophoresis</title><addtitle>ELECTROPHORESIS</addtitle><description>Micellar electrokinetic capillary chromatography (MEKC) was investigated for the determination of Viagra (sildenafil citrate, SC) and its metabolite (UK‐103,320) in human serum in a concentration range of clinical interest. For MEKC, human serum samples spiked with SC and UK were obtained directly after elution with methanol from a tC18 cartridge. The extract was evaporated and regenerated in a solution 1 mM of phosphate buffer (pH 12.3) which contained a methanol percentage of 20% that was analyzed using phosphate buffer (pH 12.3, 10 mM) containing 30 mM sodium dodecyl sulfate (SDS) as separation electrolyte and a fused‐silica capillary. This method gave satisfactory interday precision with respect to migration times relative standard deviation (RSD < 1%) and linear responses for the concentration ranges investigated (0.50–3.50 mg L–1 for the compound SC and 0.90–4.60 mg L–1 for UK). An intraday RSD (n = 5 graphs) between the slopes of the calibration graphs was acceptable (6.40%) for SC and (3.37%) for UK. A satisfactory interday precision between slopes was also obtained (RSD 4.10% for SC and a RSD 2.72% for UK) which demonstrated the ruggedness of this method. Detection limits (S/N = 3) were about 200 ng/mL for both compounds in human serum. MEKC was shown as a good method with regards to simplicity, precision and sensitivity.</description><subject>Electrophoresis, Capillary - methods</subject><subject>Electrophoresis, Capillary - statistics & numerical data</subject><subject>Human serum</subject><subject>Humans</subject><subject>Male</subject><subject>Micellar electrokinetic capillary chromatography</subject><subject>Micelles</subject><subject>Osmolar Concentration</subject><subject>Phosphodiesterase Inhibitors - blood</subject><subject>Phosphodiesterase Inhibitors - metabolism</subject><subject>Piperazines - blood</subject><subject>Piperazines - metabolism</subject><subject>Purines</subject><subject>Pyrimidinones - blood</subject><subject>Pyrimidinones - metabolism</subject><subject>Sildenafil Citrate</subject><subject>Sildenafil citrate (Viagra)</subject><subject>Sildenafil metabolite (UK-103</subject><subject>Sildenafil metabolite (UK‐103,320)</subject><subject>Sodium Dodecyl Sulfate</subject><subject>Sulfones</subject><subject>Temperature</subject><issn>0173-0835</issn><issn>1522-2683</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2001</creationdate><recordtype>article</recordtype><sourceid>EIF</sourceid><recordid>eNqVUU1vEzEUXCEQDYW_gHxCrcSG54_9ChVSSUupCASVQgQXy9l925juroPtFeTEX8dLQjhx4GTNe-MZeyaKTiiMKQB7RhPGYpbm_IgBUEiPGZtQOAlATCanl2fx-ez9hwG94GMYT-fPWby4E4321-5GI6AZjyHnyUH0wLmvEMiFEPejA0pFmoiiGEU_3-oSm0ZZgg2W3ppb3aHXJSnVWg_zDSlX1rTKmxur1qsNqY0lfoWkQo-21Z3y2nTE1OSTVoFCVFcR7R1p0aulabRHcvTxTUyBP-UMjonuyKpvVUcc2r59GN2rVePw0e48jK5fnV9PX8ez-cXl9HQWlyKnIk6TmimkSVUpkSmg-TJTNUfIVLmsGWdhwWmdA2XA80IUWZqJkouCYi2qVPDD6MlWdm3Ntx6dl612vz_eoemdzCiwNOEJ3_uX1jhnsZZrq9sQg6Qgh17kELAcApbbXmSAYTc0IWXoRf7pRXIJcjqXTC6C7OOdf79ssforuisiED5vCd91g5v_Mv2H534WtOOttnYef-y1lb2VacazRC7eXcgivbp6efaFh8f-AsIPtp4</recordid><startdate>200106</startdate><enddate>200106</enddate><creator>Nevado, Juan J. Berzas</creator><creator>Flores, Juana Rodríguez</creator><creator>Peñalvo, Gregorio Castañeda</creator><creator>Fariñas, Nuria Rodríguez</creator><general>Wiley Subscription Services, Inc., A Wiley Company</general><scope>BSCLL</scope><scope>CGR</scope><scope>CUY</scope><scope>CVF</scope><scope>ECM</scope><scope>EIF</scope><scope>NPM</scope><scope>AAYXX</scope><scope>CITATION</scope><scope>7X8</scope></search><sort><creationdate>200106</creationdate><title>Micellar electrokinetic capillary chromatography for the determination of Viagra and its metabolite (UK-103,320) in human serum</title><author>Nevado, Juan J. Berzas ; Flores, Juana Rodríguez ; Peñalvo, Gregorio Castañeda ; Fariñas, Nuria Rodríguez</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c4814-65f2ae15dda47a018b7af3e07acbf2325dd31f80120389497674c3491ef4d643</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2001</creationdate><topic>Electrophoresis, Capillary - methods</topic><topic>Electrophoresis, Capillary - statistics & numerical data</topic><topic>Human serum</topic><topic>Humans</topic><topic>Male</topic><topic>Micellar electrokinetic capillary chromatography</topic><topic>Micelles</topic><topic>Osmolar Concentration</topic><topic>Phosphodiesterase Inhibitors - blood</topic><topic>Phosphodiesterase Inhibitors - metabolism</topic><topic>Piperazines - blood</topic><topic>Piperazines - metabolism</topic><topic>Purines</topic><topic>Pyrimidinones - blood</topic><topic>Pyrimidinones - metabolism</topic><topic>Sildenafil Citrate</topic><topic>Sildenafil citrate (Viagra)</topic><topic>Sildenafil metabolite (UK-103</topic><topic>Sildenafil metabolite (UK‐103,320)</topic><topic>Sodium Dodecyl Sulfate</topic><topic>Sulfones</topic><topic>Temperature</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Nevado, Juan J. Berzas</creatorcontrib><creatorcontrib>Flores, Juana Rodríguez</creatorcontrib><creatorcontrib>Peñalvo, Gregorio Castañeda</creatorcontrib><creatorcontrib>Fariñas, Nuria Rodríguez</creatorcontrib><collection>Istex</collection><collection>Medline</collection><collection>MEDLINE</collection><collection>MEDLINE (Ovid)</collection><collection>MEDLINE</collection><collection>MEDLINE</collection><collection>PubMed</collection><collection>CrossRef</collection><collection>MEDLINE - Academic</collection><jtitle>Electrophoresis</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Nevado, Juan J. Berzas</au><au>Flores, Juana Rodríguez</au><au>Peñalvo, Gregorio Castañeda</au><au>Fariñas, Nuria Rodríguez</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Micellar electrokinetic capillary chromatography for the determination of Viagra and its metabolite (UK-103,320) in human serum</atitle><jtitle>Electrophoresis</jtitle><addtitle>ELECTROPHORESIS</addtitle><date>2001-06</date><risdate>2001</risdate><volume>22</volume><issue>10</issue><spage>2004</spage><epage>2009</epage><pages>2004-2009</pages><issn>0173-0835</issn><eissn>1522-2683</eissn><abstract>Micellar electrokinetic capillary chromatography (MEKC) was investigated for the determination of Viagra (sildenafil citrate, SC) and its metabolite (UK‐103,320) in human serum in a concentration range of clinical interest. For MEKC, human serum samples spiked with SC and UK were obtained directly after elution with methanol from a tC18 cartridge. The extract was evaporated and regenerated in a solution 1 mM of phosphate buffer (pH 12.3) which contained a methanol percentage of 20% that was analyzed using phosphate buffer (pH 12.3, 10 mM) containing 30 mM sodium dodecyl sulfate (SDS) as separation electrolyte and a fused‐silica capillary. This method gave satisfactory interday precision with respect to migration times relative standard deviation (RSD < 1%) and linear responses for the concentration ranges investigated (0.50–3.50 mg L–1 for the compound SC and 0.90–4.60 mg L–1 for UK). An intraday RSD (n = 5 graphs) between the slopes of the calibration graphs was acceptable (6.40%) for SC and (3.37%) for UK. A satisfactory interday precision between slopes was also obtained (RSD 4.10% for SC and a RSD 2.72% for UK) which demonstrated the ruggedness of this method. Detection limits (S/N = 3) were about 200 ng/mL for both compounds in human serum. MEKC was shown as a good method with regards to simplicity, precision and sensitivity.</abstract><cop>Hoboken</cop><pub>Wiley Subscription Services, Inc., A Wiley Company</pub><pmid>11465499</pmid><doi>10.1002/1522-2683(200106)22:10<2004::AID-ELPS2004>3.0.CO;2-W</doi><tpages>6</tpages><oa>free_for_read</oa></addata></record> |
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| subjects | Electrophoresis, Capillary - methods Electrophoresis, Capillary - statistics & numerical data Human serum Humans Male Micellar electrokinetic capillary chromatography Micelles Osmolar Concentration Phosphodiesterase Inhibitors - blood Phosphodiesterase Inhibitors - metabolism Piperazines - blood Piperazines - metabolism Purines Pyrimidinones - blood Pyrimidinones - metabolism Sildenafil Citrate Sildenafil citrate (Viagra) Sildenafil metabolite (UK-103 Sildenafil metabolite (UK‐103,320) Sodium Dodecyl Sulfate Sulfones Temperature |
| title | Micellar electrokinetic capillary chromatography for the determination of Viagra and its metabolite (UK-103,320) in human serum |
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